CN105602598A - Collecting testing method for benzopyrene in coal asphalt - Google Patents
Collecting testing method for benzopyrene in coal asphalt Download PDFInfo
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- CN105602598A CN105602598A CN201510991945.9A CN201510991945A CN105602598A CN 105602598 A CN105602598 A CN 105602598A CN 201510991945 A CN201510991945 A CN 201510991945A CN 105602598 A CN105602598 A CN 105602598A
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- coal tar
- bap
- tar pitch
- testing
- collecting
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/08—Working-up pitch, asphalt, bitumen by selective extraction
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Civil Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Structural Engineering (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Working-Up Tar And Pitch (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention belongs to the technical field of detection of coal asphalt, in particular to a collecting testing method for benzopyrene in coal asphalt. The method comprises the steps: (1) grinding a coal asphalt sample in a mortar till all the coal asphalt fully passes by a 80-mesh sieve; (2) building a collecting device, adding a solvent for collecting into a conical flask as a collecting bottle, weighing the coal asphalt sample in a three-opening flask, regulating oil bath temperature, setting a stirring rate of a stirrer, regulating a collecting rate of an atmosphere sampler, reacting and collecting; (3) testing content of benzopyrene in the solution in the collecting bottle by a standard curve method of an ultraviolet spectrophotometer. Compared with prior art, the collecting testing method for the benzopyrene in the coal asphalt can efficiently accurately test the release amount of the benzopyrene in the coal asphalt under a heating condition, sampling is convenient to perform, an extracting progress is easy and timesaving, the used collecting device is a universal device and high in suitability.
Description
Technical field
The invention belongs to coal tar pitch detection technique field, specifically, relate to BaP in a kind of coal tar pitchCollect method of testing.
Background technology
Coal tar pitch coal tar asphalt is one of major product of coal tar deep processing, is that coal tar distillation extracts cutAfter raffinate. Under coal tar pitch normal temperature, be a kind of thermoplasticity black energy light-emitting solid material, without fixing fusing point, beGlassy phase, the chemical composition of coal tar asphalt is very complicated, and it is to encircle above many cyclophanes perfume (or spice) by kind more than 5,000 threeFamily's hydrocarbon compound and containing the heterocyclic compounds such as oxygen, nitrogenous, sulfur-bearing and a small amount of macromolecule carbon element material composition.Low-molecular-weight component has crystallinity, forms multi-component eutectic mixture.
Coal tar pitch can be used as electrode material, waterproof material and road-making material etc., at building, electrode and fire proofed woodThe field important roles such as material. But traditional coal tar pitch and asphalt have larger difference on composition,Especially pollutant aspect, the high activity carcinogenic substance BaP containing in coal tar pitch is the more than ten thousand times of asphalt.BaP claims again benzo (ɑ) pyrene, english abbreviation BaP, coal tar pitch when heating, wherein 3,4-BaP is releasedBe put in atmosphere, combine with the aerosol that in atmosphere, all kinds particulate forms, wherein below 8 μ mPart easily enters lung through respiratory tract, causes lung cancer and angiocardiopathy.
In recent years, environmental issue receives the concern in worldwide, add my coal tar pitch output large, at someAspect has irreplaceability, make people extensively think deeply research how by carcinogenic substances such as BaPs wherein from coal dropIn green grass or young crops, separate or control, thereby preparing the coal tar pitch of low toxicity, asepsis environment-protecting. And to its method of testingResearch be top priority. In current method of testing, be mostly directed to solid coal tar pitch BaP at normal temperaturesContent test, and coal tar pitch is while using as road-making material, processes, mix and stir, making and rolling allUnder heated condition, therefore, when normal temperature, its BaP content can not characterize coal tar pitch and makes as road-making materialThe harm of its BaP of used time, lacks directive significance to production application; In addition on the one hand, benzo in atmosphereIn pyrene assay, exist the shortcomings such as sampling difficulty, extraction procedure complicated and time consumption.
Summary of the invention
For solving the problems of the technologies described above, the invention provides benzene in the coal tar pitch of a kind of succinct convenience, efficiently and accuratelyAnd the collection method of testing of pyrene.
The collection method of testing of BaP in a kind of coal tar pitch of the present invention, described collection method of testing is concreteStep is: 1) coal tar pitch sample is ground in mortar, extremely all coal tar pitch are completely by 80 mesh sieveTill; 2) build gathering-device, in the conical flask as receiving flask, add to collect and use solvent 100mL, take100-300g coal tar pitch sample is placed in there-necked flask, regulates oil bath temperature, and the stir speed (S.S.) of agitator is set,Adjust the acquisition rate of air sampler, reaction, collection 30-120min; 3) by the solution in receiving flask, adoptTest the wherein content of BaP with the calibration curve method of ultraviolet specrophotometer.
The collection method of testing of BaP in a kind of coal tar pitch of the present invention, described step 2) in, collect and useSolvent is the one in benzene, toluene, acetone.
The collection method of testing of BaP in a kind of coal tar pitch of the present invention, described step 2) in, collect and useSolvent is two kinds in benzene, toluene, acetone.
The collection method of testing of BaP in a kind of coal tar pitch of the present invention, described step 2) in, collect and useSolvent is benzene, toluene and acetone, and three's mol ratio is 5:3:2.
The collection method of testing of BaP in a kind of coal tar pitch of the present invention, described step 2) in, collect and useSolvent is benzene, toluene and acetone, and three's mol ratio is 5:4:1.
The collection method of testing of BaP in a kind of coal tar pitch of the present invention, described step 2) in, regulate oilBath temperature is 50～150 DEG C.
The collection method of testing of BaP in a kind of coal tar pitch of the present invention, described step 2) in, agitatorMixing speed be 100～2000r/min.
The collection method of testing of BaP in a kind of coal tar pitch of the present invention, described step 2) in, atmosphere is adoptedThe sampling rate of sample device is 100～1000mL/min.
The collection method of testing of BaP in a kind of coal tar pitch of the present invention, described step 3) in, adopt purpleOuter spectrophotometric calibration curve method is tested the wherein content of BaP.
The collection method of testing of BaP in a kind of coal tar pitch of the present invention, described step 1) in, by coal dropBlue or green 22 β-acetyl group Glycyrrhiza Uralensis saponin(e C mixed grinding pulverizing with accounting for quality 0.5%.
Compared with prior art, in coal tar pitch of the present invention, the collection method of testing of BaP can be at fire-barUnder part, test efficiently and accurately the burst size of BaP in coal tar pitch, and sampling is convenient, extraction procedure is simple and easy saves time,Its gathering-device used can be fexible unit, strong adaptability.
Detailed description of the invention
Below in conjunction with specific embodiment to the collection method of testing of BaP in coal tar pitch of the present invention do intoOne step explanation, but protection scope of the present invention is not limited to this.
Embodiment 1
Taking domestic certain producer's medium temperature coal pitch as raw material, coal tar pitch is ground, until all by 80 objectsTill sieve; Build gathering-device, in the conical flask as receiving flask, add to collect and use solvent 100mL, collectWith solvent be benzene; Take 100g asphalt powder, be positioned in 1000mL there-necked flask, regulate oil bath heating-up temperatureBe 90 DEG C, mixing speed 1000r/min, air sampler sampling rate is 1.0L/min, collection liquid is benzene, adoptsSample 1 hour, reaction finishes, and stops heating and stirs. Question response device is cooled to room temperature, gets sample in receiving flask,Adopt ultraviolet specrophotometer to test wherein BaP content. While adopting this course of reaction and parameter, in coal tar pitchBaP burst size is 0.52%.
Embodiment 2
Taking domestic certain producer's medium temperature coal pitch as raw material, coal tar pitch is ground, until all by 80 objectsTill sieve; Build gathering-device, in the conical flask as receiving flask, add to collect and use solvent 100ml, collectThe benzene that is equimolar ratio with solvent and toluene; Take 200g asphalt powder, be positioned in 1000mL there-necked flask,Regulating oil bath heating-up temperature is 100 DEG C, mixing speed 1000r/min, and air sampler sampling rate is 0.8L/min,Collection liquid is benzene, samples 1.5 hours, and reaction finishes, and stops heating and stirs. Question response device is cooled to chamberTemperature, gets sample in receiving flask, adopts ultraviolet specrophotometer to test wherein BaP content. Adopt this to reactWhen journey and parameter, in coal tar pitch, BaP burst size is 0.58%.
Embodiment 3
Taking domestic certain producer's medium temperature coal pitch as raw material, coal tar pitch is ground, until all by 80 objectsTill sieve; Build gathering-device, in the conical flask as receiving flask, add to collect and use solvent 100mL, collectWith solvent be acetone; Take 300g asphalt powder, be positioned in 1000mL there-necked flask, regulate oil bath to add hot temperatureDegree is 120 DEG C, mixing speed 1500r/min, and air sampler sampling rate is 0.8L/min, collects liquid to beBenzene, samples 2 hours, and reaction finishes, and stops heating and stirs. Question response device is cooled to room temperature, gets receiving flaskMiddle sample, adopts ultraviolet specrophotometer to test wherein BaP content. While adopting this course of reaction and parameter,In coal tar pitch, BaP burst size is 0.75%.
Embodiment 4
Taking domestic certain producer's medium temperature coal pitch as raw material, coal tar pitch is ground, until all by 80 objectsTill sieve; Build gathering-device, in the conical flask as receiving flask, add to collect and use solvent 100ml, collectWith solvent be benzene, toluene and acetone, three's mol ratio is 5:3:2; Take 100g asphalt powder, be positioned over 1000mLIn there-necked flask, regulating oil bath heating-up temperature is 100 DEG C, mixing speed 1000r/min, air sampler sampling speedRate is 0.6L/min, and collection liquid is benzene, samples 1 hour, and reaction finishes, and stops heating and stirs. Question responseDevice is cooled to room temperature, gets sample in receiving flask, adopts ultraviolet specrophotometer to test wherein BaP content.While adopting this course of reaction and parameter, in coal tar pitch, BaP burst size is 0.61%.
Embodiment 5
Taking domestic certain producer's medium temperature coal pitch as raw material, coal tar pitch is ground, until all by 80 objectsTill sieve; Build gathering-device, in the conical flask as receiving flask, add to collect and use solvent 100ml, collectWith solvent be benzene, toluene and acetone, three's mol ratio is 5:4:1; Take 200g asphalt powder, be positioned over 1000mLIn there-necked flask, regulating oil bath heating-up temperature is 120 DEG C, mixing speed 1500r/min, air sampler sampling speedRate is 1.0L/min, and collection liquid is benzene, samples 2 hours, and reaction finishes, and stops heating and stirs. Question responseDevice is cooled to room temperature, gets sample in receiving flask, adopts ultraviolet specrophotometer to test wherein BaP content.While adopting this course of reaction and parameter, in coal tar pitch, BaP burst size is 0.78%.
Embodiment 6
Taking domestic certain producer's medium temperature coal pitch as raw material, coal tar pitch is ground, until all by 80 objectsTill sieve; Build gathering-device, in the conical flask as receiving flask, add to collect and use solvent 100ml, collectWith solvent be benzene, toluene and acetone, three's mol ratio is 5:3:2; Take 300g asphalt powder, be positioned over 1000mLIn there-necked flask, regulating oil bath heating-up temperature is 120 DEG C, mixing speed 1000r/min, air sampler sampling speedRate is 1.0L/min, and collection liquid is benzene, samples 2 hours, and reaction finishes, and stops heating and stirs. Question responseDevice is cooled to room temperature, gets sample in receiving flask, adopts ultraviolet specrophotometer to test wherein BaP content.While adopting this course of reaction and parameter, in coal tar pitch, BaP burst size is 0.76%.
Embodiment 7
Taking domestic certain producer's medium temperature coal pitch as raw material, coal tar pitch is ground, until all by 80 objectsTill sieve; Build gathering-device, in the conical flask as receiving flask, add to collect and use solvent 100ml, collectWith solvent be benzene, toluene and acetone, three's mol ratio is 5:4:1; Take 100g asphalt powder, be positioned over 1000mLIn there-necked flask, regulating oil bath heating-up temperature is 100 DEG C, mixing speed 1000r/min, air sampler sampling speedRate is 1.0L/min, and collection liquid is benzene, samples 1.5 hours, and reaction finishes, and stops heating and stirs. Treat anti-Should be cooled to room temperature by device, get sample in receiving flask, adopt ultraviolet specrophotometer to test wherein BaP content.While adopting this course of reaction and parameter, in coal tar pitch, BaP burst size is 0.63%.
Embodiment 8
Taking domestic certain producer's medium temperature coal pitch as raw material, coal tar pitch is ground, until all by 80 objectsTill sieve; Build gathering-device, in the conical flask as receiving flask, add to collect and use solvent 100ml, collectWith solvent be benzene, toluene and acetone, three's mol ratio is 5:3:2; Take 200g asphalt powder, be positioned over 1000mLIn there-necked flask, regulating oil bath heating-up temperature is 90 DEG C, mixing speed 1600r/min, air sampler sampling speedRate is 1.0L/min, samples 2 hours, and reaction finishes, and stops heating and stirs. Question response device is cooled to room temperature,Get sample in receiving flask, adopt ultraviolet specrophotometer to test wherein BaP content. Adopt this course of reaction andWhen parameter, in coal tar pitch, BaP burst size is 0.92%.
Embodiment 9
Taking domestic certain producer's medium temperature coal pitch as raw material, coal tar pitch is ground, until all by 80 objectsTill sieve; Build gathering-device, in the conical flask as receiving flask, add to collect and use solvent 100ml, collectWith solvent be benzene, toluene and acetone, three's mol ratio is 5:4:1; Take 300g asphalt powder, be positioned over 1000mLIn there-necked flask, regulating oil bath heating-up temperature is 90 DEG C, mixing speed 1200r/min, air sampler sampling speedRate is 1.0L/min, and collection liquid is toluene, samples 2 hours, and reaction finishes, and stops heating and stirs. Treat anti-Should be cooled to room temperature by device, get sample in receiving flask, adopt ultraviolet specrophotometer to test wherein BaP content.While adopting this course of reaction and parameter, in coal tar pitch, BaP burst size is 0.89%.
Embodiment 10
Taking domestic certain producer's medium temperature coal pitch as raw material, by coal tar pitch and the 22 β-acetyl group Ural that accounts for quality 0.5%Glycyrrhizin C mixed grinding is pulverized, until all by 80 object sieves; Build gathering-device, in conductIn the conical flask of receiving flask, add to collect and use solvent 100ml, collection is benzene, toluene and acetone with solvent, and three rubsYou are than being 5:3:2; Take 200g mixed-powder, be positioned in 1000mL there-necked flask, regulate oil bath heating-up temperatureBe 90 DEG C, mixing speed 1600r/min, air sampler sampling rate is 1.0L/min, samples 2 hours, reactionFinish, stop heating and stir. Question response device is cooled to room temperature, gets sample in receiving flask, adopts ultraviolet to divideLight photometer is tested wherein BaP content. While adopting this course of reaction and parameter, in coal tar pitch, BaP dischargesAmount is 1.07%.
Embodiment 11
Taking domestic certain producer's medium temperature coal pitch as raw material, coal tar pitch and the Tea Saponin mixed grinding that accounts for quality 0.5% are pulverized,Until all by 80 object sieves; Build gathering-device, in the conical flask as receiving flask, add receiptsCollection solvent 100ml, collection is benzene, toluene and acetone with solvent, three's mol ratio is 5:3:2; Take 200gMixed-powder, is positioned in 1000mL there-necked flask, and regulating oil bath heating-up temperature is 90 DEG C, mixing speed1600r/min, air sampler sampling rate is 1.0L/min, samples 2 hours, reaction finishes, and stops heatingAnd stirring. Question response device is cooled to room temperature, gets sample in receiving flask, adopts ultraviolet specrophotometer to test itMiddle BaP content. While adopting this course of reaction and parameter, in coal tar pitch, BaP burst size is 0.86%.
Claims (9)
1. a collection method of testing for BaP in coal tar pitch, is characterized in that, described collection method of testing toolBody step is: 1) coal tar pitch sample is ground in mortar, extremely all coal tar pitch are completely by 80 mesh sievesTill son; 2) build gathering-device, in the conical flask as receiving flask, add to collect and use solvent 100mL, claimGet 100-300g coal tar pitch sample and be placed in there-necked flask, regulate oil bath temperature, the stir speed (S.S.) of agitator is set,Adjust the acquisition rate of air sampler, reaction, collection 30-120min; 3) by the solution in receiving flask, adoptTest the wherein content of BaP with the calibration curve method of ultraviolet specrophotometer.
2. the collection method of testing of BaP in a kind of coal tar pitch according to claim 1, is characterized in that,Described step 2) in, collection is the one in benzene, toluene, acetone with solvent.
3. the collection method of testing of BaP in a kind of coal tar pitch according to claim 1, is characterized in that,Described step 2) in, collection is two kinds in benzene, toluene, acetone with solvent.
4. the collection method of testing of BaP in a kind of coal tar pitch according to claim 1, is characterized in that,Described step 2) in, collection is benzene, toluene and acetone with solvent, three's mol ratio is 5:3:2.
5. the collection method of testing of BaP in a kind of coal tar pitch according to claim 1, is characterized in that,Described step 2) in, collection is benzene, toluene and acetone with solvent, three's mol ratio is 5:4:1.
6. the collection method of testing of BaP in a kind of coal tar pitch according to claim 1, is characterized in that,Described step 2) in, adjusting oil bath temperature is 50-150 DEG C.
7. the collection method of testing of BaP in a kind of coal tar pitch according to claim 1, is characterized in that,Described step 2) in, the mixing speed of agitator is 100-2000r/min.
8. the collection method of testing of BaP in a kind of coal tar pitch according to claim 1, is characterized in that,Described step 2) in, the sampling rate of air sampler is 100-1000mL/min.
9. the collection method of testing of BaP in a kind of coal tar pitch according to claim 1, is characterized in that,Described step 3) in, adopt the calibration curve method of ultraviolet specrophotometer to test the wherein content of BaP.
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| CN201510991945.9A CN105602598B (en) | 2015-12-25 | 2015-12-25 | The collection test method of BaP in a kind of coal tar pitch |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5413533A (en) * | 1977-07-04 | 1979-02-01 | Kawatetsu Kagaku Kk | Method of reducing 3*4 benzpyrene in coal tar pitch |
| CN1536054A (en) * | 2003-04-07 | 2004-10-13 | 王福恒 | Method for producing coal pitch by utilizing coal solvent and adopting continuous leaching-out process and its leaching-out equipment |
| CN104403681A (en) * | 2014-11-26 | 2015-03-11 | 辽宁石油化工大学 | Method for extracting benzopyrene from coal pitch |
| CN104458483A (en) * | 2014-12-17 | 2015-03-25 | 常熟市苏常工程质量检测有限公司 | Exhaust gas detection device for batch preparation plant of chemical factory |
| CN104479714A (en) * | 2014-11-26 | 2015-04-01 | 辽宁石油化工大学 | Method for efficiently separating benzopyrene in coal pitch |
-
2015
- 2015-12-25 CN CN201510991945.9A patent/CN105602598B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5413533A (en) * | 1977-07-04 | 1979-02-01 | Kawatetsu Kagaku Kk | Method of reducing 3*4 benzpyrene in coal tar pitch |
| CN1536054A (en) * | 2003-04-07 | 2004-10-13 | 王福恒 | Method for producing coal pitch by utilizing coal solvent and adopting continuous leaching-out process and its leaching-out equipment |
| CN104403681A (en) * | 2014-11-26 | 2015-03-11 | 辽宁石油化工大学 | Method for extracting benzopyrene from coal pitch |
| CN104479714A (en) * | 2014-11-26 | 2015-04-01 | 辽宁石油化工大学 | Method for efficiently separating benzopyrene in coal pitch |
| CN104458483A (en) * | 2014-12-17 | 2015-03-25 | 常熟市苏常工程质量检测有限公司 | Exhaust gas detection device for batch preparation plant of chemical factory |
Non-Patent Citations (1)
| Title |
|---|
| 谢志强: "《企业污染控制与绿色经营实务全书》", 31 October 2000, 中国环境科学出版社 * |
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